A TECHNICAL REPORT ON

STUDENTS’ INDUSTRIAL WORK EXPERIENCE SCHEME

(SIWES)
UNDERTAKEN AT
GRACELAND ANALYTICAL LABORATORY, NO 4 IGWEBUIKE
STREET AWKA, ANAMBRA STATE
BY
EBEDE, CHIDIEBELE FAVOUR
(2019544043)
DEPARTMENT OF PURE AND INDUSTRIAL CHEMISTRY, FACULTY OF
PHYSICAL SCIENCES, NNAMDI AZIKIWE UNIVERSITY, AWKA,
ANAMBRA STATE.

IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR THE

AWARD OF BACHELOR OF SCIENCE (B.Sc.) DEGREE IN PURE AND
INDUSTRIAL CHEMISTRY.

JUNE, 2023

1
 DEDICATION
I dedicate this report to God Almighty for his sufficient grace in my academic
journey and also to my Late Dad, Mr. Chidiebele Charles Ebede who has always
prayed for a day like this in my life.

2
 ACKNOWLEDGEMENT
I appreciate God Almighty for his direction, guidance and provision towards my
academics.
I also thank the Management of Graceland Analytical Laboratory Limited, Awka
led by the Director, Dr Onyebuchi Nwadiogbu, the manger and my industrial based
supervisor Mrs Nwosu Mirabel, for accepting for me to train with them for the
period of my Industrial training.
Special thanks also to Dr Nkechi Okoye HOD, Pure and Industrial Chemistry,
Nnamdi Azikiwe University and my lecturers for the exceptional teachings and
academic tutelage.
I thank in a very special way my ever supportive family starting with my
wonderful Mom, Mrs. Charity Ngozi Ebede, my amicable Mentor Mrs.
Amaraugochukwu Ogunoegbunam and to my siblings, Chidera and Ifeanyi for
their immense love that kept me going.
I also thank my Uncles and Wives who supported me through this journey
especially Sir &Lady Azubike Clara Mgbenu , Mr and Mrs. Ugochukwu Ebede,
Mr Ugochukwu & Obinna Onyenwe and Barr. & Lady Roland Ebele Mgbenu, I
can't possibly mention all but I thank you all for the amazing role played regarding
my education.
I also appreciate the VUMEF family directed by Sen. Victor Umeh for the
unending support as regards to my education.

3
 ABSTRACT
This industrial training report is centred on the work done and experience gained
during my six months of the training undertaken at Graceland Analytical
Laboratory Limited Awka, Anambra state from November, 2022 through May,
2023. It also provides inclusive information about the SIWES program such as its
history, objectives and aims while also giving a description of the work done in
Graceland Analytical Laboratory Limited. It further focuses on the various
laboratory researches and analysis on production of activated charcoal, proximate
analysis, phytochemical analysis and water analysis carried out in the laboratory. It
finally gives a few recommendations on how to further improve the SIWES
program

4
 TABLE OF CONTENTS
1. Dedication……………………………………………………2

2. Acknowledgement…………………………………………,,,3

3. Abstract………………………………………………………4

4. Table of content………………………………………………5

5. List of Figures………………………………………………....6

6. Chapter One (Introduction)…………………………………..7

7. Chapter Two (Literature review)…………………………….10

8. Chapter Three (Job description)……………………………..13

9. Chapter Four (conclusion and recommendation)……….......38

10.Citation and Referencing……………………………………..39

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 LIST OF FIGURES
Figure 1……………………………………..Organizational chart
Figure 2……………………………………Coconut shells
Figure 3…………………………………….Coconut charcoal
Figure 4……………………………………Activated charcoal
Figure 5…………………………………….Soxhlet extractor set up
Figure 6…………………………………….Photometer
Figure 7…………………………………….Secchi disc
Figure 8…………………………………….BOD Bottle
Figure 9…………………………………….Weighing Balance
Figure 10…………………………………...Conductivity meter
Figure 11……………………………………Drying of orange leaves
Figure 12…………………………………….Preparation of the binder
Figure 13………………………………Preparation of sample mixture with binder
Figure 14…………………………………….Ejection of produced solid fuel

6
 CHAPTER ONE
INTRODUCTION
1.1 Background of SIWES
The Students Industrial Work Experience Scheme (SIWES) is a Skills Training
Programme designed to prepare and expose Students of Universities, Polytechnics,
Colleges of Education, Colleges of Technology and Colleges of Agriculture for the
Industrial Work situation they are likely to meet after graduation.
The Scheme affords Students the opportunity of familiarizing and exposing
themselves to handling equipment and machinery that are usually made available
in their institutions.
Before the establishment of the Scheme, there was a growing concern that
graduates of our institutions of higher learning lacked adequate practical
knowledge and that the theoretical education in higher institutions was not
responsive to the needs of the Employer's of Labour.
It is against this background that the Industrial Training Fund(ITF) initiated,
designed and introduced SIWES Scheme in 1973 to acquaint Students with the
skills of handling industrial equipment and machinery.
The Industrial Training Fund(ITF) solely funded the Scheme during its formative
years. However, due to financial constraints, the Fund withdrew from the Scheme
in 1978. The Federal Government noting the significance of the skills training
handed the management of the Scheme to the National Universities

7
Commission(NUC) and the National Board for Technical Education(NBTE) in
1979. In November, 1984 the management and implementation of the Scheme was
reverted again to the ITF with the funding to be solely borne by the Federal
Government.

1.2Objectives of SIWES
The objectives of SIWES among others include to:
1. Provide an avenue for students in institution of higher learning to acquire
industrial skills and experience in their various course of study.
2. To make the transition from school tom the world of work easier and to enhance
students contacts for later job placement.
3. Expose Students to work methods and techniques in handling equipment and
machinery that may not be available in their institutions.
4. To enlist and strengthen employers involvement in the whole education process
of preparing university graduates for employment after graduation.
5. Provide students the opportunity to see the real world of their discipline, apply
their theoretical knowledge and consequently bridge the gap between theory and
practice.
1.3 Scope of the technical report
This report seeks to provide a better, environmental and economic friendly
approach to activated carbon production, phytochemical analysis, proximate
analysis and water analysis. It will also provide an ideal technology to utilize and
convert Plantain peels/waste into valuable products i.e activated carbon which can
be commercialized for the removal of contaminants from aqueous phase.

1.4 Significance of SIWES

8
 It brings about better academic studies as students have realized that theories
in class have application on the field.
 It strengthens the employers in involvement in the entire educational process
of training or preparing university and polytechnic graduates for
employment in the industries.
 The scheme is target at bridging the gap between theories and practical
which makes the student better graduate for the Nation.
 The experience acquired during the industrial work experience training will
go a long way in preventing or reducing industrial hazards which may have
resulted from mishandling of equipment and machinery in the industries.

9
 CHAPTER TWO
LITERATURE REVIEW
2.1 Brief History of Graceland Analytical Laboratory Limited.
Graceland analytical laboratory limited was registered in 2016 as a
nongovernmental laboratory that offers analytical and research services to
individuals and organization in the area of food, beverages, soil, water, plants and
other products aiming to request the highest quality and accuracy of testing level
which will refresh the spirit of competition among manufacturers, employees and
above all, will be 100% for the benefits of both national and international
customers
VISION STATEMENT
To build a responsive service oriented, strong and visible organization with
customer friendly hall mark and commitment on excellence in a bid to restructure
the expectation of a brighter future
MISSION STATEMENT
To become the first real indigenous research laboratory with national states that
employs self motivated, skilled and professionals who are always at the cutting
edge with efficiency, cost effective and environmental friendly solution in science
and technology
DIRECTORATES AND THEIR FUNCTIONS
BOARD OF DIRECTOR
1. Responsible for all activites including lab activites and staff
10
 2. Responsibility as pertains to the laboratory

3. Takes administrative decisions for the lab policy

4. Provides laboratories with the required human and financial resources that
are require by the lab director to carry out the laboratory process

LABORATORY DIRECTOR
1. Responsible for admistration of all laboratory activitie and staff

2. Responsible in taking decisions with repect to laboratory policy and

resources

3. Responsible for laboratory’s human and financial resources that are adequate
for the laboratory processes.

4. Approves the qulity manual

5. Requests the result needed to participate in the proficiency testing scheme

6. Takes decision to participate in the proficiency testing scheme in the field of

his dministration

7. Undertake the management reviews of management system

8. Ensure the appropriate communication to check the effectiveness of the

management system

9. Appoints technical managers and quality manager

10. Appoints their deputies when absent

11.Maintains the management system and ensure that it is implemented inside

the lab

11
 12.Evaluation of the quality management system, its maintenance and
improvement

13. Ensure that the human and financial resources are adequate for the
laboratory process

14.Approves the management and technical procedures

15.Ensure the training of key pesonsimplemented according to the training plan

16.Approves the laboratory developed methods

17.Management representative to ensure quality management is established,

implemented and maintained in the laboratory

2.2Organizational chart and organogram

BOARD OF DIRECTOR

DIRECTOR

QUALITY MANAGER

TECHNICAL MANAGER

QUALITY LAB ANALYST

LAB TECHNICIANS ADMINISTRATIVE

SECRETARY CLEANER

Fig 1: Organizational chart

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 CHAPTER THREE
JOB DESCRIPTION
3.1 Production of activated charcoal
Activated charcoal is a form of carbon with an increased surface area for
adsorption. It also referred to as activated carbon, activated coal or active charcoal,
a carbon source is treated under certain conditions to increase its surface area
and/or its number of pores. On an average, the estimated surface area for a gram of
activated charcoal is about 500 square meters.(Ningthoujam S.,2010)
3.1.1 Material and equipment
Any organic material such as plantain peels, or hardwood (charcoal) can be used as
precursor or raw materials (provided it’s a non toxic carbon source with absorbent
properties), burning sink, oven, 25% conc. CaCl 2or ZnCl2, sterilized water, plastic
pail, draining tray, zipper bag and blender.
3.1.2 Procedure
The coconut/plantain shells was stripped off, washed thoroughly and allowed to
dry completely. If drying is not done properly, they may be difficult to burn. Add
the dried coconut shells in the burning sink by adjusting the temperature to about
600-900oF. The temperature range was maintained and burnt continuously for
about 41/2 hours or until the coconut shells turn into ash. Allow to cool for safe
handling. The ash was carefully taken out of the sink and transferred into a clean
plastic pail. 25% conc. CaCl2 was added such that the ash was soaked completely.
The pail was covered with a lid and left for about 24 hours. During this process,
the chemicals were impregnated into the ash, after which further treatment will
13
transform the ash into activated charcoal. The charcoal was removed from the pail
and transferred into a draining tray and allowed to drain for an hour.
For removal of any trace chemicals from the charcoal, the charcoal was washed
and rinsed repeatedly with sterilized water. Thorough washing is essential in order
to get rid of the chemical solution. After washing, keep the charcoal in the tray for
draining water; transfer the charcoal into an oven setting the temperature to about
215-230oF and bake for about 3 hours. After baking, the activated charcoal was
removed from the oven and crushed with the help of a blender or a hammer and
stored in zipper bags for future use.

Fig.2: coconut shells Fig.3: coconut charcoal Fig.4: activated charcoal

3.1.3 Benefits of activated charcoal

Activated charcoal is thought to offer so many benefits which include:
1. For Emergency poison treatment: the toxin-binding property of the carbon
aids in reducing the effects of the poisoning (Bond, G.R, 2002). It can be used
in cases of prescription and over-the-counter medication overdoses
(Albertson, T. E et al, 2011).

2. For kidney health improvement: the absorbing nature of activated charcoal

14
 may aid in promoting the kidney function. By reducing the number of waste to
be filtered, it reduces the kidney’s filtering task. Activated charcoal binds the
toxins and waste which will be excreted through faeces (Musso, C. G.et al,
2010).

3. For treating fish odour syndrome: Activated charcoal helps reduce the
trimethyaminuria (fish odour syndrome) concentration in the body (Yamazaki,
H et al, 2004).

4. To alleviate bloating and gas: A study conducted in the American Journal of

Gastroenterology proves the application of activated charcoal in reducing gas
and bloating (Jain, N. K, 1986).

5. For skin cleansing

6. For mould cleansing

7. For digestive cleansing.

3.2 Extraction and phytochemical analysis of paw paw leaf

3.2.1 Materials Required
In phytochemical extraction of plant phytochemicals the following equipment’s are
used
Soxhlet Extractor: This is a glass equipment consisting of a condenser, extractor
chamber and thimble extractor.
Heating mantle: This use as a source of heat supply which can be regulated to
different temperature
Retort stand: This is a science equipment use as clamp to provide support in

15
holding a device in a vertical position.

Fig.5:soxhlet extractor setup

The reagents were used namely, Hydrochloric acid, Meyer’s reagent, Wagner’s
reagent, NaOH, ferric chloride, Conc H 2SO4, Fehling’s solution, acetic anhydride,
methanol,SDA culture media.
3.2.2 Preparation and extraction of samples
The samples were dried under room temperature for and grounded into powder.The
samples were soak in 500ml extraction solvent(methanol) for 24-hour then transfer
into a soxhlet extractor then extracted for about an hour.

3.2.3 Phytochemical screening of the Plant samples

The phytochemical tests below were carried out on paw paw water extract to
determine the active constituents. These phytochemical tests were done to detect
the presence of secondary metabolites, such as alkaloids, tannins, saponins, resins,
flavonoids, steroid, glycosides and terpenoids in the plant under investigation.
3.2.3.1 Test for Alkaloids
A quantity (3ml) of the sample was boiled with 5ml of 2% HCl on a steam bath.
The mixture was filtered and 1ml portion of the filtrate was measured into three
test tubes. Each of the 1ml filtrate was treated with 2 drops of the following
reagents.
i. Dragendorff’s Reagent: A red precipitate indicates the presence of alkaloids.
ii. Mayer’s Reagent: A creamy-white colour precipitate indicates the presence of

16
alkaloids.
iii. Wagner’s Reagent: A reddish-brown precipitate indicates the presence of
alkaloids.
3.3.3.2 Test for Flavonoids
Three millilitres of the extracts was treated with 1 ml of dilute NaOH. The
presence of a cloudy precipitate confirms the presence of flavonoids.
3.2.3.3 Test for Glycosides
Dilute sulphuric acid (5ml) was added to 4ml each of the extracts in a test tube and
boiled for 15 minutes in a water bath. It was then cooled and neutralized with 20%
potassium hydroxide solution. A mixture, 10ml of equal parts of Fehling’s solution
A and B was added and boiled for 5 minutes. A more dense red precipitate
indicates the presence of glycoside.
3.2.3.4 Test for Steroids
2ml of acetic anhydride were added to 3ml extract of each sample with the
addition of 2ml H2SO4. A colour change from violet to blue or green indicated the
presence of steroids

3.2.3.5 Terpenes (Liebermann-Burchard reaction)

To 2 ml extract, 2ml acetic anhydride and few drops concentrated sulphuric acid
were added in a test tube. Blue-green ring between layers indicates the presence of
steroids and pink- purple ring indicates the presence of terpenes.
3.2.3.6 Test for Saponins
Five (5ml) of distilled water was added to 2 ml of the extracts in a test tube and
shaken vigorously. The formation of foams or stable frothing following the shaking
indicated the presence of saponins
3.2.3.7 Test for cardiac glycoside (Keller-killiani’s test)
2 ml of 3% ferric chloride solution was added to the extract and allowed to stand
17
for one minutes. 1ml of conc. H 2SO4 was carefully drop down the wall of the tube
so as to form a lower layer. A reddish brown ring at the interface indicated the
presence cardiac glycoside.
3.2.3.8 Anthraquinones
Two milliliters of 10% hydrochloric acid were added to the extract in a test tube
and boiled for about two minutes. Equal amount of chloroform was added to the
test tube and vortexes twice, the chloroform layer was pipette out and then equal
volume of 10% ammonia was added. A pinkish red colour observed in upper layer
indicated the presence of anthraquinones.
3.2.3.9 Test for Saponin glycosides
To 3ml of the extract, 3ml of fehling’s solution A and B was added. A bluish green
precipitate showed the presence of saponin glycosides.
3.2.3.10 Tests for volatile oils
One 1ml of the fraction was mixed with dil. HCL. A white precipitate was formed
which indicated the presence of volatile oils.
3.2.3.11 Test for Tannins(Ferric Chloride Test)
A quantity (2ml) each, of the extracts was boiled with 5ml of 45% ethanol for 5
minutes. Each of the mixtures was cooled and filtered. The different filtrates were
subjected to the following tests. A quantity (1ml) each of the filtrates was diluted
with distilled water and added 2 drops of ferric chloride. A transient greenish to
black colour indicates the presence of tannins.
3.2.3.12 Test for Acidic Compounds
A quantity (1ml) each of the extracts was placed in a clear dry test tube and
sufficient water added. These were warmed differently in a hot water bath and
cooled. A piece of water-wetted litmus paper was dipped into the different filtrates
and observed for colour change. Acidic compounds turn blue litmus paper red.
3.2.3.13 Test for Resins
18
Two tests were carried out to detect the presence of resins in the plant under
investigation.
i. Precipitate Test
A quantity (2ml) each of the extracts was treated with 15ml of 96% ethanol. The
alcoholic extract was then poured into 20ml of distilled water in a beaker. A
precipitate occurring indicates the presence of resins.
ii. Color Test
A quantity (3ml) each of the extracts was treated with chloroform and the extracts
concentrated to dryness. The residues were re-dissolved in 3ml of acetone and 3ml
of concentrated hydrochloric acid added. The mixtures were now heated differently
in a water bath for 30 minutes. Pink color, which changes to magenta-red, indicates
the presence of resins.

3.3 Proximate Determination

The proximate determination or analysis of local bread, fresh pepper, and common

beans were determined in the laboratory.

The following materials were used in the proximate analysis: Test tubes, Test tube

rack, Soxhlet extractor ,Conical Flask, Pipette, Electric blender , Heating mantle,

Fume cupboard, weighing balance, silica dish, funnel, filter paper, oven, petri dish,

thimble, retort stand and muffle furnace.

The reagents used include: Concentrated sulphuric acid, Dilute hydrochloric acid,

distilled water, Ethanol, Acetic anhydride, Ferric Chloride, Petroleum ether,

sodium hydroxide, boric acid, methylene indicator, sodium sulphate, kjeldahl

19
catalyst, copper sulphate, selenium speck, crucible, acetone, phenolphthalein,

indicator, ammonia, molybidic acid.

3.3.1 Moisture content determination

A measured weight of the fresh sample (5g) was put in a previous weighed

moisture can and dried in the oven at 95-100 0C under pressure not exceeding

100mgHg for 30 minutes in the first instance. It was cooled on the desiccators and

reweighed. The weight was recorded and the sample returned to the oven for

further drying. The drying, cooling and weighing was done at intervals and

repeatedly until a constant weight was obtained. By weight difference, the weight

of moisture lost was determined and expressed as a percentage of the sampled

weight analyzed.

It was calculated using the formula:

Moisture (%) =
W1= initial weight of empty crucible

W2= weight of empty crucible + sample

W3= final weight of empty crucible + sample after drying to constant weight

3.3.2 Ash content determination.

The furnace incineration gravimetric method was used. A measured weight (5g) of

each sample was put in a previously weighed porcelain crucible. The sample in the

crucible was put in a muffle furnace at 550 0C for 2 hours, the sample was allowed

20
to burn until it became white ash. The crucible was carefully removed from the

furnace (taking care not to allow air blow the ash away), cooled in the desiccator

and reweighed. The difference in weight of ash was obtained and expressed as

percentage of the sample weight analyzed. The ash content of the sample was then

calculated using the formula:

Ash (%) =
Where;

W = weight of sample

W1 = weight of empty crucible

W2 = weight of crucible + ash

3.3.3 Crude fiber determination

This was determined by the Wende method. 5g of the each sample were defatted

(fat determination) using petroleum ether. The defatted samples were boiled in

200mls of 1.25g of H2S04 solution under reflux for 30 minutes. After that, the

sample was washed with several portions of hot water using a two-fold muslin

cloth to trap the particles. The washed samples were carefully transferred back to

the flask and 200ml of 1.25% NaOH solution was added to it. Again the samples

was boiled for 30 minutes and washed with hot water. It was then carefully

transferred to a weighed porcelain crucible and dried in the oven at 105°C for an
21
hour, cooled in desiccators and was reweighed. The loss in weight after

incineration was used to determine the crude fiber content and expressed as a

percentage of the weight of the samples.

Crude fibre was calculated as follows:

Crude fiber (%) =

Where;

W1 = weight of sample

W2 = weight of crucible + sample after drying

W3 = weight of crucible + sample ash.

3.3.4 Fat Content determination

The continuous solvent extraction method using a soxhlet extractor was used. 2g of

each sample were wrapped with a weighed porous paper (Whatmann filter paper

No 40). The wrapped samples were put in a soxhlet reflux flask. This flask was

mounted onto a weighed oil extraction flask containing 300ml of petroleum ether

(40-60°C boiling points). The upper end of the reflux flask was connected to a

condenser. The solvent in the extraction flask was heated using an electro thermal

heater. The vaporized solvent condensed into the reflux flask and completely

covered the wrapped samples. The samples remained in contact with the solvent

until the flask filled up and siphoned over thereby carrying extracted oil (fat) down

to the boiling flask. The cycle of vaporization, condensation, extraction, and reflux

22
was allowed to go in interrupted (repeatedly) for about 4 hours before the defatted

samples were carefully brought out with the aid of forceps and the solvent

recovered leaving the oil extract. The defatted wrapped samples was further dried

in the oven at 100°C for 1 hour, cooled in a desiccator and weighed. The

experiment was repeated two or more times to get an average. The fat content was

determined by weight difference of each sample and expressed as a percentage of

each weight of sample as shown below:

Fat (%) =
Where;

W1 = weight of empty filter paper

W2 = weight of paper + sample before defatting

W3 = weight of paper + sample after defatting and drying.

3.3.5 Crude protein determination

The protein content of the samples was determined by the kjeldahl method. The

total nitrogen was determined and multiplied by the factor 6.25 to obtain the

protein content; 0.5g of each sample was mixed with 10ml of concentrated

sulphuric acid (H2SO4) in a kjeldahl digestion flask. A tablet of a selenium catalyst

was added to it and the mixture was digested by heating in a fume cupboard until a

clear solution was obtained. Each of the digest was carefully transferred into a

100ml volumetric flask and made up to the mark by distilled water. A 10ml portion

of each digest was mixed an equal volume of 45% NaOH solution in a kjeldahl
23
distilling unit. The mixture was distilled and the distillate collected into 10ml of

4% boric acid solution containing three drops of mixed indicator-bromocresol

green and methyl red. A total of 50mls distillate was collected and titrated against

0.02N H2SO4 solution from green to a deep red point. A reagent blank was also

digested, distilled and the titrated, just as the sample. The nitrogen and protein

content was calculated thus:

Nitrogen (%) =

Where;

W = weight of sample analyzed

N = Normality of titrant (0.02N)

T= Titre value

14= Molar mass of Nitrogen

The percentage of protein was calculated as % protein = %nitrogen × 6.25.

3.3.6 Carbohydrate content determination:

The carbohydrate content of the test samples was determined by estimation using

the arithmetic difference method. The carbohydrate was calculated and expressed

as the nitrogen free extract (NFE) as shown below:

% CHO (Nitrogen free extract) = 100 - %[Moisture + Ash+Fat+Protein].

3.4 WATER ANALYSIS

24
3.4.1 Equipment

The equipment’s used include, burrette, heating mantle, magnetic stirrer and

shaker, 250ml and 250 beakers, 250ml conical flask, timer, digital weighing

balance, Buchner funnel, Digital thermometer, calibrated secchi disk, pH meter, pH

paper, digital electrical conductivity meter, 50ml BOD bottle, stopper, Whatman

filter paper N0:41, heating flask, porcelain dish and photometer.

and photometer.

Fig.6: photometer Fig. 7: secchi disc Fig.8: BOD bottle

Fig.9: weighing balance Fig.10: conductivity meter

3.4.2 Reagents

The reagent used include alkali iodide-azide reagent, H 2SO4, sodium thiosulphate

25
solution ,starch indicator, methyl red indicator ,EDTA salt, NaOH, boric acid,

HCL, acetic acid, phenoldisulphonic, KOH and NH4OH.

3.4.3 Procedure for Physicochemical Parameter of Water(WHO, 2004)

The physicochemical parameter of water checked include, temperature,

transparency, conductivity, total dissolved oxygen, total dissolved solid, pH, total

suspended solid, alkalinity and acidity, chloride concentration, water hardness

calcium and magnesium concentration, Nitrogen and Nitrate.

3.4.3.1 Temperature: 5mL of the water sample from the three stations was

measured with a measuring cylinder into 250ml beaker. Digital thermometer was

inserted and allowed to stand on it for 1min. The reading were taken and recorded

for each sample. The procedure was repeated twice times and the average reading

taken and recorded.

3.4.3.2 Transparency and Turbidity: calibrated hygrometer disc was inserted in

the water body from the point of collection. The point at which the disc disappears

from sight was noted and recorded and the point at which it reappears again was

also noted and recorded. Transparency/ turbidity were calculated as follows.

Secchi disc transparency/turbidity(cm) =

Where
A = Depth at which secchi disc disappear
B = Depth at which secchi disc reappear

3.4.3.3 pH: The pH was determined using a pH meter in conjunction with pH

26
paper. 5ml of the sample was measure and the pH meter calibrated using

calibrating solution of pH then inserted into the sample and allowed for 2min

before reading was taken. pH paper was also used to confirm the reading as well.

3.4.3.4 Conductivity: 5mL of the sample was measure into 250ml beaker and

digital electrical conductivity meter was inserted into the sample and the reading

recorded for the three stations respectively.

3.4.3.5 Total Dissolved Oxygen (Modified Winkler’s Method)

5mL of water sample were measure into 50ml BOD bottle followed by 2ml alkali

iodide-azide reagent yellow precipitate appear indicating the presence of

dissolved oxygen(DO). A stopperwas fitted into the BOD bottle to carefully

exclude air bubble and was vortex for 10times. The precipitate was allowed to

settle down and 2ml concentrated H 2SO4 was added then vortex until the

precipitate completely got dissolved.

20ml of the sample was titrated against 0.025N sodium thiosulphate solution to a

pale yellow colour in a presence of 1ml starch indicator and the titration continued

until the disappearance of blue colour. The titre value was calculated as follows

DO(mg/l) =
Where; V = Volume of acid
N = Normality of Na2S2O3
3.5.3.6 Total Dissolved Solid (Gravimetric Method)
50ml of each sample were measure and filtered through Whatman filter paper

N0:41 into 250ml heating flask pre-heated at 105 0c. The filtrate was further heated
27
on a hot plate to dryness then allowed to cool. Total dissolved solid was calculated

as for follow;

Total dissolved solid(TDS)mg/l =

Where,

W1 = Initial weight of beaker

W2 = Final weight beaker

V = volume of sample

3.4.3.7 Total suspended solid (Gravimetric Method)

Pre dried filter paper was used to filter 50ml of each samples. The filter paper was

then dried in oven and the total suspended solid calculated as follow.

Total suspended solid (mg/l) = ...........11

Where,

W1 = Initial weight of filter paper

W2 = Final weight filter paper

V = volume of sample

3.4.3.8 Alkalinity and Acidity

3ml of the sample was measured into 150ml beaker and pH paper with calibration

value from 1-14 with acidity and alkalinity calibration. The reading for the samples

were taken and recorded respectively.

3.4.3.9 Water Hardness (Ca and Mg) (Titrimetric Method)

50ml of the sample was measure into 250ml conical flask. The pH was raised to12

by adding 2ml NaOH. A drop of methyl red indicator was added and titrated with
28
10ml EDTA until the colour change from purple to pink. Water hardness was

calculated as

Calciumhardness CaCO3(mg/l) = x 1000..........12

Magnesium hardness = total hardness – calcium hardness
Calcium hardness (mg/l) = calcium hardness as CaCO3 x0.40
Magnesium hardness(mg/l) = magnesium hardness x0.243

Where
A= ml of EDTA used
B=mg CaCO3 equivalent to 1ml EDTA

3.4.3.10 Nitrogen (Titrimetric Method)

To30ml of the sample, 10ml and 15ml anhydrous sodium sulphate and copper

sulphate was added. 10ml H2SO4 was added then heat on a hot plate for 30min. the

sample was allowed to cool and 15ml NaOH was added before distillation.

Ammonia was then trapped in 20ml boric acid during the distillation process and

titrated against 0.02N of HCl in the presence of methyl red indicator. Nitrogen was

calculated as follows

Nitrogen =
Where;
T= titre value
0.02 = Normality of HCl used
V = volume of sample used

3.4.3.11 Nitrate(Photometric Method): To 100ml of each sample, acetic acid was

added to bring the pH to 7. 50ml of each of adjusted sample was measured into a

porcelain disk and evaporated to dryness over a water bath. 2ml of

29
phenoldisulphonic acid reagent was used to dissolve the residue. 10ml of distil

water was added and shake to dissolve. 10ml of KOH was added followed by 4ml

of NH4OH solution to avoid turbidity. The sample was allowed to stand for

20minutes for colour development. Photometer was use to check for the

absorbance of the sample at 410nm alongside it blank. The absorbance reading was

compared with that of the standard solution of nitrate and recorded accordingly for

each sample.

3.4.3.12 Chorine (Titrimetric method): to 2 ml of each sample, 3ml of acetic

acid was added to reduce the pH to 4 or below 4. 1gm of potassium iodide was

added and the sample titrated against standard sodium thiosulphate until colour

change to yellow. 1ml of starch solution was added and it was further titrated until

blue colour disappeared. Chlorine concentration was calculated as

Free chlorine as Cl2(mg/l) =

Where,
A= ml titration for sample
B=ml titration for blank
N =normality of sodium thiosulphate used

3.4.3.13 BOD(Iodometric method): 2ml each of the water sample was measured

into BOD bottle and 1ml of phosphate buffer Magnesium sulphate calcium

chloride and iron (iii) chloride was added 2% dilution of glucose glutamic acid was

also added. Dissolved oxygen in one of the BOD bottle was measured alone side

the blank on the first day. The other replicated sample were incubated for 5 days at

30
the temperature of 200c and after which the dissolved oxygen of the incubated

replicated water sample was measured along with the blank was measured and

BOD calculate as

BOD(mg/L) =
Where,
D1 = Dissolve Oxygen simple initially
D2 = Dissolve oxygen of diluted sample after incubation
P=decimal volumetric fraction of sample

3.5 Briquette production

The process of making a briquette is by mixing the material with a binder or

adhesive. It involves compaction of biomass residue into a uniform solid fuel.

Potential agricultural biomass materials which can be used include: orange,

pawpaw, mango or cashew leaves, corn cobs, mango leaves, walnut shells (Jin and

wang, 2011).

Equipment Used: The Equipment used includes briquette moulder, mixer, conical

flask, thermometer, sieve, digital weighing balance, blender and timer.

Reagents Used: The reagent used include distilled water and Binder (cassava

starch)

3.5.1 Sample Preparation/Pre-Treatment

The sample (orange leaves) was grounded into powdery form using a blender.

The ground sample was sieved through a 2mm sieve to achieve a homogeneous

size. The pre-treatment include: sorting, drying, size reduction, calcinations and

31
maceration.

3.5.1.1 Sorting: The feedstock was carefully sorted manually to remove

impurities such as pieces of wood, bone, metal and any other unwanted materials.

3.5.1.2 Drying: the samples was air dried to reduce the moisture content (up to

90% dryness) and then they will be evenly mixed and oven dried at 50 0C and the

local starch used as binder will be air dried at room temperature for 48h.

3.5.1.3 Size Reduction: The biomass wasreduced in size by milling until it could

pass through a screen or reaches a suitably small and uniform size (1 mm). The

hair waste being very light will be reduced to 0.5 mm.

3.5.1.4 Calcination:500g of each of the dried samples was put in a crucible and

placed in an oven at a temperature of 450 0C for 30 min. The calcined samples will

then be transferred into a silver plate to reduce the temperature and avoid further

combustion.

3.5.1.5 Maceration: The waste was macerated to provide uniform consistency

(slurry). This will be done by mixing equal amounts of each sample with cassava

starch and water at the ratio of 4:5:1. The cassava starch will be heated to melt it

and will be mixed with samples so as to facilitate flow of lignin present in the

biomass, which acts as a natural binder to increase adhesion between

intermolecular particles.

32
 Fig.11: drying of orange leaves fig. 12: preparation of the binder

Fig.13:preparation of sample mixture with binder Fig. 14:

ejection of the produced solid fuel

3.5.2 Characterization of briquette

3.5.2.1 Moisture content: Moisture content of the briquette samples was

determined based on sample weight measurement before and after oven drying

(Adekunle et al., 2015) The initial weight of the samples were determined (W 1) and

placed in an oven set at 105±3°C for 24hours. The samples were removed and

cooled in a desiccators, and reweighed (W 2). Percentage moisture content will be

calculated as in equation 1 below

Percentage moisture =

33
 Where,
W1 = weight of sample before oven drying, (g) W 2 = weight

of oven dried sample, (gram)

3.5.2.2 Volatile Matter (method of Adekunle et al): The briquettes percentage

volatile matter content was determined using Lenton furnace. The residue of dry

sample from moisture content determination preheated at 300°C for 2hrs to

drive off the volatiles, the resulting sample will be further heated at 470°C 2hrs,

to ensure complete elimination of volatiles, just before the materials turn to

ashes, and then cooled in desiccator. The crucible with known weight and its

content will be weighed and expressed as the percentage weight loss, the

percentage volatile matter will be computed using equation 2.

Volatilematter = …….2

3.5.2.3 Fixed Carbon Content: The Fixed carbon will be determined by using the

data previously obtained from volatile matter and ash content analysis and

according to equation.

%FC = 100 – %(ash + volatile matter)

3.5.2.4 Ash Content (method of Adekunle et al., 2015): Ash content of the

samples briquettes was determined using a furnace residue from fixed carbon

determination were heated in a furnace at 590°C, for two hours and transferred into

34
a desiccators and allowed to cool down, the materials turned into white ash and

weighed. Same procedure was repeated three time at 1hr interval until the weight

was constant. The weight was recorded as the final weight of the ash. The

percentage ash content will be calculated using equation.

3.5.2.5 Density (method of ASTM, 1990):The density was determined using a

weighing balanced in the laboratory by taking the weight of briquette sample and

the dimension measurement using vernier caliper, the volume will be evaluated

using the relation nr2h and the density was computed using equation

3.5.2.6 Determination of Afterglow Time:The determination of afterglow time is

done in order to estimate how long the individual briquette will burn before

restocking when used in cooking and heating (Oladeji, 2010). A piece of oven-

dried briquette will be ignited and after a consistent flame is established, the flame

will be blown out. The time, in seconds, within which the glow was perceptible

will be recorded.

3.5.2.7 Combustibility Test (method of Onuegbu et al., 2011): 150g of each set

of briquettes will be stacked into an improved stove. It will be lightened with a

match after application of little absolute ethanol to initiate combustion. The fire

will be allowed to assume a steady combustion. One litre of water in an aluminum

pot whose initial temperature was recorded will be placed on the stove and a stop

watch will be initiated. A digital thermometer will be inserted into the water inside

35
the pot and readings taken after every two minutes interval and the corresponding

temperatures recorded until water boiled

3.5.2.8 Water Resistance Capacity of Dry Briquette

Percentage of water resistance capacity of dry briquette wascarried out by

immersing dry briquette in 500ml beaker glass container containing distilled water

at 29 ± 2∘C for 120 seconds. The Relative change in weight of the briquette will be

measured. Percentage water gain will be calculated using the following

relationship in equation 6.

%water gained by briquette =

Where;

1= Initial weight of briquette before immersion

2 = Final weight of briquette after immersion.

Hence, water resistance capacity% = 100% − %water absorbed.

3.5.2.9 Shattering index (durability index) was determined according to

ASTMD440-86 (1998): Each briquette produced will be dropped from a height of

2meter. The weight of the briquette before shattering and after shattering will be

recorded. The shattering index will be calculated as in equation 7

Shattering index=

3.5.2.10 Burning Rate

Briquette burning rate was determined according to the method used by Onuegbu
36
et al (2012).The insulator, Bunsen burner, tripod stand and wire gauze will be

arranged on the balance and their weight recorded. Briquette sample of known

weight was placed on wire gauze and the burner ignited. This will be positioned on

top of a mass balance monitored to record instantaneous measurements of the mass

every 10 seconds throughout the combustion process using a stopwatch, until the

briquettes will be completely burnt and constant weight was obtained. The weight

loss at specific time will be computed from the expression in equation 8

Burning Rate =
3.5.3 Applications of Briquettes

Briquettes are used for domestic and industrial purposes in both rural and urban

areas. They serve as a developmental intervention to replace firewood, charcoal, or

other solid fuels because current scarcities and rising prices of fuel has made

consumers to look for affordable alternatives (Oladeji, 2015).

37
 CHAPTER FOUR
CONCLUSION AND RECOMMENDATIONS
4.1 Conclusion
My six months industrial training at Graceland Analytical Laboratory Limited has
been one of the interesting, productive, instructive, and educative experiences in
my life. The whole experience gained during the attachment was very enlightening.
The practical skills we were exposed to and the opportunity to relate with typical
situations relating to chemical laboratory which successfully broadened my
understanding and interest in pure and industrial chemistry as a profession. The
training has it accorded to me the privilege of gaining insight into job preparation
as well as what it meant to carry out proper laboratory analysis and researches and
also working condition under stress which in a way prepares undergraduates for the
outside world after school.
The program gave me the privilege to relate with senior professionals and my
fellow students.
4.2 Recommendations
Although SIWES has and is still achieving quite a lot of its stated objectives,
nevertheless the following recommendations are suggested to improve the
qualitative context of the program:
1. Proper orientation should be given to the students by the university before
they go on SIWES at least before mid-semester of the first semester.
2. The placement letter should be given to the students early enough so as to
avoid attachment in irrelevant organisation.
3. Industries and firms should be persuaded to accept students on training as
most of them reject students without any reason.
4. Allowance should be paid during the period of the training so as to allow
students take care of some financial issues.
38
 CITATION AND REFERENCING

REFERENCES

Adekunle, J. O., J. S. Ibrahim, and E. I. kucha., (2015). Proximate and ultimate

analysis of biocoal briquette of Nigerian’s Ogboyaga and Okaba sub-
bituminuos coal. Current journal of Applied Science and Technology,7(1):
114-123.
Albertson, T. E, Owen, K. P., Sutter, M E., &Chan, A. L. (2011). Gastrointestinal
deconatamination in the acutely poisoned patient international journal of
emergency medicine, 4(1), 65
American Society for Testing and Materials (ASTM. D440-86)( 1998), “Standard
test method of drop shatter test for coal,” in Annual Book of ASTM
Standards, 05: 188–191, West Conshohocken,Pa, USA,.
ASTM 1990, Annual Book of ASTM standards; Petroleum products, lubricants,
and Fossil fuels, Vol. 5 (part 5); Gaseous Fuels, coal and coke, D3173-87,
pp. 310-312.
Bamgboye A. and Bolufawi, S. (2018) “Physical characteristics of briquettes
fromGuinea corn (sorghum bi-color) residue,” Agricultural Engineering
International, article 1364.
Bond, G. R. (2002). The role of activated charcoal and gastric emptying in
gastrointestinal decontamination; a state-of-the-art review. Annals of
emergency medicine, 39(3), 273-286
Brunerová R., and Brožek.,E((2016)Characterization of woodstove briquettes from
torrefied biomass and coal. Energy, 171, 853–865.
Enig,N and Fallon,T(2010)Trease and Evans Pharmacognosy (15th edn), Elsevier
Science limited, New York, pp 156-200.
Felfli M.N.,Muazu, R.I.; Stegemann, J.A.(2011) Operating variables on durability

39
 of fuel briquettes from rice husks and corn cobs. Fuel Process. Technol.
133, 137–145.
Jain, N. K., Patel, V. P., & Pitchumoni, C. S., (1986). Efficacy of Activated
charcoal in Reducing Intestinal Gas: A Double-Blind Clinical Trial.
American Journal of Gastroenterology, 81(17).
Jin, Z. Q., and S. X. Wang (2011) specific energy requirement for compacting corn
cobs. Advanced material research, 148, 245-252.
Musso, C. G., Michelangelo, H., Reynaldi, J., Patel, E., & Clark, R. F. (2015). A
retrospective review of the prehospital use of activated charcoal. The
Ameerican journal of emergency medicine, 33(1), 56-59.
Ningthoujam, S., (2010) How to make activated charcoal.
https://www.buzzle.com/articles/how-to-make-activated-charcoal.html. ss
Oladeji, T., (2015). Characteristics of some biomass briquette prepared under
modest die pressures. Biomass Bioenergy 18, 223-228
Onuegbu, T. Ekpunobi, U U. E.. Ogbu I. M,. Ekeoma, M.O and Obumselu, F.
O(2012). “Comparative studies of ignition time and water boiling test of
coal and biomass briquettes blend,” International Journal of Research &
Reviews in Applied Sciences, 7:153–159.
Onuegbu, T. U. (2010). Improving Fuel Wood Efficiency in Rural Nigeria, (A Case
of Briquette Technology). International Journal of Chemistry in Nigeria:
3(4): 35-39.
Onuegbu, T. U., Ekpunobi, U. E., I. M., Ekeoma, M. O. and Obumselu, F. O.
(2011). Comparative studies of Ignition time and Water boiling Test of Coal
and Biomass Briquettes Blend. IJRRAS, 7 (2): 153- 159.
Reynolds, W.C,(2012)Trease and Evans Pharmacognosy (13th edn), W.B. Saunder
Company limited, USA, pp 100-120.
Rinaldi,M (2009)Modern coconut management. Food and Agriculture
40
 Organization (FAO), Rome, p 458.
Silva, E( 2013).Replanting the tree of life (coconut): Towards an international
agenda of coconut palm research, C.A.B. international, Wallingford, UK, p
156.
World Health Organization (2004) Guidelines for drinking-water quality (3rd
edition)
Yamazi, H., Fujieda, M., Togashi, M., Saito, T., Preti, G., Cashman, J. R., &
Kamataki, T. (2004). Effects of the dietary Supplements, activated charcoal
and copper chlorophyllin, on urinary excretion of trimethylamine in
Japanese trimethylaminuria patients. Life Sciences, 74(22), 2739-2747.

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